CN104480317A - Cobalt nickel metallurgy wastewater sludge recycling method - Google Patents

Cobalt nickel metallurgy wastewater sludge recycling method Download PDF

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CN104480317A
CN104480317A CN201410639327.3A CN201410639327A CN104480317A CN 104480317 A CN104480317 A CN 104480317A CN 201410639327 A CN201410639327 A CN 201410639327A CN 104480317 A CN104480317 A CN 104480317A
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acid
cobalt
manganese
nickel
reaction
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CN104480317B (en
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朱蕾
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SHAOXING KEQIAO DRAIN CO., LTD.
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朱蕾
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention provides a cobalt nickel metallurgy wastewater sludge recycling method, and belongs to the field of waste recycling. The method comprises the following steps: carrying out acid dissolution reduction on cobalt nickel metallurgy wastewater sludge to leach out valuable metals in the wastewater sludge, displacing copper by using manganese powder to recover copper, precipitating zinc by using manganese sulfide to recover zinc, using a fluoride to remove calcium and magnesium from the obtained zinc removed solution, carrying out advanced impurity removal and cobalt nickel manganese enrichment by using a P2O4 extractant, and carrying out advanced impurity removal on the obtained solution rich in cobalt, nickel and manganese by using manganese sulfide to obtain a solution for preparing an NCM ternary precursor. The method allows nickel, cobalt, manganese, zinc, copper and other metals to be completely recovered and the obtained cobalt, nickel and manganese solution to be used to prepare the NCM ternary precursor as a raw material, avoids cobalt, nickel and manganese separation, and also has the advantages of simple process, substantial improvement of the metal recovery rate, low cost, harmlessness to environment, and industrialization prospect.

Description

A kind of cobalt metallurgy of nickel waste water slag recycling processing method
Technical field
The present invention relates to utilization of waste as resource field, be specifically related to a kind of cobalt metallurgy of nickel waste water slag recycling processing method.
Background technology
Along with the continuous exploitation of cobalt nickel raw ore, the utilization of cobalt nickel secondary resource is subject to people's attention day by day, the waste water containing cobalt nickel produced in cobalt nickel hydrometallurgy and cobalt nickel product preparation process, the cobalt nickel waste water slag produced after wastewater treatment, because it contains cobalt, nickel, copper, zinc, the heavy metals such as manganese, how the focus that recycling treatment become people to pay close attention to is carried out to it, also be problem in the urgent need to address, according to production experience, cobalt 3000 tons/year, the hydrometallurgy factory of 1500 tons/year, nickel, the cobalt nickel waste water slag of annual generation about 1000 tons, metal values is wherein up to nearly ten million.
For the process of cobalt metallurgy of nickel waste water slag, general processing mode has 2 kinds, and a kind of is add sulfide after reduction of dissolved by precipitated metals such as nickel cobalt copper wherein and enrichment, then obtains the raw material of high-grade nickel cobalt copper through sulfurization roasting.This technique can only recycle nickel, cobalt, copper in waste water slag, and sulfurization roasting environmental pollution is too large.Another is fire reduction melting, waste water slag is added carbon and obtains polymetallic metal sheet in high temperature reduction melting, then through electrochemical dissolution recovery metal wherein.This technical process is long, and cost is high.
Summary of the invention
Propose a kind of technique of this waste water slag of recycling treatment herein, the metals such as nickel cobalt MnZn copper can reclaim by this technique completely, the cobalt nickel manganese solution simultaneously obtained can be used as the raw material of preparation NCM ternary precursor, avoid the separation of cobalt nickel manganese, technique is more simple, and metal recovery rate improves greatly, and cost is low, environmental sound, has the prospect of industrialization.
Concrete technology principle is as follows:
1. reducing leaching.Main component due to waste water slag is precipitate metal hydroxides, and it exposes in atmosphere and following reaction can occur:
Co(OH) 2+2H 2O+O 2=Co(OH) 3
Mn(OH) 2+O 2=MnO 2+2H 2O
Leach so need add after trivalent cobalt and tetravalent manganese are reduced into divalence by reductive agent, for S-WAT, the chemical equation that reducing leaching occurs is as follows:
2Co(OH) 3+2H 2SO 4+Na 2SO 3=2CoSO 4+5H 2O+Na 2SO 4
MnO 2+2H 2SO 4+Na 2SO 3=MnSO 4+H 2O+Na 2SO 4
2Fe(OH) 3+2H 2SO 4+Na 2SO 3=2FeSO 4+5H 2O+Na 2SO 4
2M(OH) 3+2H 2SO 4=2M 2(SO 4) 3+6H 2O
(M be Al, Cr etc. three valence state metal)
M(OH) 2+H 2SO 4=MSO 4+H 2O
(M is the divalent state metals such as Zn, Cu, Ni, Ca, Mg)
Solution after dissolving is the metal ion such as deironing aluminium chromium again, and for sodium chlorate and sodium hydroxide, the chemical equation that deironing aluminium chromium etc. occur is as follows:
6FeSO 4+12NaOH+NaClO 3+3H 2O=NaCl+6Fe(OH) 3+6Na 2SO 4
M 2(SO 4) 3+ 6NaOH=2M (OH) 3+ 3Na 2sO 4(M be Al, Cr etc. three valence state metal)
2. manganese powder displacement.Because the lively type of manganese is higher than copper, so manganese powder can copper in substitutional solution, its chemical equation occurred is as follows:
Mn+CuSO 4=Cu+MnSO 4
3. manganese sulfide dezincifies.Because the solubleness of zinc sulphide is far below manganese sulfide, therefore can remove zine ion with manganese sulfide, the chemical equation of its reaction is as follows:
MnS+ZnSO4=MnSO4+ZnS
4. Sodium Fluoride calcium-magnesium removing.Because the solubleness of Calcium Fluoride (Fluorspan), magnesium fluoride is less, therefore available fluoride carrys out removal of impurities, and for Sodium Fluoride, the chemical equation of its reaction is as follows:
CaSO 4+2NaF=CaF 2+Na 2SO 4
MgSO 4+2NaF=MgF 2+Na 2SO 4
5.P204 extracting and enriching.P204 extraction agent by the metal ion in the aqueous solution as cobalt nickel mn ion is extracted in organic phase from water, then can control comparing of back extraction, thus obtains the nickel cobalt manganese solution of high density, and sodium ion etc. stay in aqueous.
6. the manganese sulfide degree of depth dezincifies.Because P204 also by enrichments such as zinc-coppers, can cause the content of zinc and copper in strip liquor higher, do nickel-cobalt-manganternary ternary anode material higher for impurity element requirements such as zinc-coppers, so manganese sulfide deep impurity-removing need be used again.
Compare conventional sulfide precipitation-roasting method process waste water slag, decrease the discharge of the sulfurous gass such as sulfurous gas, simultaneously energy synthetical recovery various metals, technical process is short, and equipment is simple, and metal recovery rate is high, and cost is low.
The technical solution used in the present invention is as follows:
A kind of cobalt metallurgy of nickel waste water slag recycling processing method, is characterized in that: comprise following step:
1) reducing leaching.According to solid-to-liquid ratio 1:2-6 by waste water slag pulp, add the pH1-2 that acid maintains reaction, add reductive agent according to cobalt manganese mol ratio 1:0.5-4 simultaneously, stirring reaction 1-3 hour at 50-70 DEG C, oxygenant is added according to iron mol ratio 1:0.1-0.6, add the pH3.5-5.5 of alkali regulator solution, stir after 1-4 hour and filter;
2) manganese powder displacement copper.Filtrate after removal of impurities is added acid for adjusting pH 1-3, adds manganese powder according to copper mol ratio 1:1.05-1.5, maintain temperature of reaction 40-80 DEG C, stirring reaction 1-3 hour;
3) manganese sulfide dezincifies.Filtrate after copper removal is added acid and maintain reaction pH1-3, add manganese sulfide according to zinc mol ratio 1:1.1-1.5, temperature of reaction 40-80 DEG C, react after 1-3 hour and filter;
4) fluorochemical calcium-magnesium removing.Solution after dezincifying alkaline solution maintains the pH3-6.5 of solution, adds fluorochemical, maintain filtration in temperature of reaction 50-90 DEG C, stirring reaction 1-3 hour according to calcium magnesium mol ratio 1:1.2-2.0;
5) P 20 4extracting and enriching.Get P 20 4extraction agent (10-30%P204+70-90% sulfonated kerosene), use alkaline solution saponification, saponification degree 50-75%, with the extraction of separating funnel simulation 6-9 stage countercurrent, the washing of 4-6 stage countercurrent, the back extraction of 8-10 stage countercurrent, charging pH3.5-5.5, wash the sulfuric acid of acid for 0.5mol/l, sour regurgitation is the sulfuric acid of 2mol/l, feed liquid: P204: wash acid: sour regurgitation=1:4-8:0.1-0.3:0.4-0.8(volume flow ratio);
6) the manganese sulfide degree of depth dezincifies.By P 20 4filtrate after enrichment adds sulfuric acid and maintains reaction pH 1-3, adds manganese sulfide, temperature of reaction 50 DEG C, react after 1-3 hour and filter according to zinc-copper mol ratio 1:5.
In described step 1, acid is at least one in sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid, reductive agent is at least one in sulfurous acid, sulphite, oxygenant is at least one in hydrogen peroxide, oxymuriate, oxygen, and alkali is at least one in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor;
In described step 2, acid is at least one in sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid;
In described step 3, acid is at least one in sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid;
In described step 4, alkali is at least one in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor, and fluorochemical is at least one in Potassium monofluoride, Sodium Fluoride, Neutral ammonium fluoride, hydrogen fluoride;
In described step 5, alkali is at least one in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows:
1. the metals such as nickel cobalt MnZn copper can reclaim by this technique completely, and the slag as deironing aluminium can be used as cement raw material, thus has reclaimed the metallic elements such as iron aluminium wherein.Manganese powder displacement obtains copper powder thus has reclaimed copper wherein, and the manganese sulfide sulfuration cadmia obtained that dezincifies is higher-grade zinc raw material thus has reclaimed zinc wherein, and the ternary liquid finally obtained has reclaimed nickel Co-Mn metal element wherein.
2. it is LiNixCoyMn (1-x-y) O2(NCM that the cobalt nickel manganese solution obtained can be used as preparation) the raw material of ternary precursor, avoid the separation of cobalt nickel manganese, technique is more simple, and metal recovery rate improves greatly.
Cost is low, environmental sound, does not substantially produce castaway slag, has the prospect of industrialization.
Accompanying drawing explanation
Accompanying drawing is process flow sheet of the present invention.
Embodiment
Following table is waste water slag composition
Waste water slag composition %
Co Ni Cu Mn Zn Ca Mg Fe Al Cr Na
1.0 3.5 1.8 9.5 4.8 6.9 4.2 0.4 0.3 0.1 20.1
Cd Pb
0.02 0.01
According to solid-to-liquid ratio 1:3 by waste water slag pulp, add the pH1.5 that sulfuric acid maintains reaction, add S-WAT according to cobalt manganese mol ratio 1:1 simultaneously, stirring reaction 1.5 hours at 70 DEG C, solution after dissolving is the metal ion such as deironing aluminium chromium again, adds sodium chlorate and adds sodium tetraphenylborate according to iron mol ratio 1:0.02, add about the pH4.0 of liquid caustic soda regulator solution according to iron mol ratio 1:0.3, stir after 1.5 hours and filter, after deironing, liquid composition is as following table.
Liquid composition g/l after deironing
Co Ni Mn Cu Zn Mg Na Ca Other
3.3 10.1 28.5 5.4 14.9 13.8 65 0.6 ≦0.01
Filtrate after removal of impurities is added sulfuric acid and regulate pH2.0, add 100 object manganese powders and the Tetramethylammonium hydroxide according to copper mol ratio 1:0.2 according to copper mol ratio 1:1.1, maintain temperature of reaction 60 DEG C, stirring reaction 2 hours, filter, copper powder composition is as following table.
Copper powder composition %
Cu Mn Ni Co Zn
95.6 3.5 0.1 0.11 0.05
Filtrate after copper removal is added sulfuric acid and maintain reaction about pH1.5, add manganese sulfide, temperature of reaction 50 DEG C according to zinc mol ratio 1:1.2, react after 2 hours and filter, after dezincifying, liquid and dezincification slag ingredient are as following table.
Liquid composition g/l after dezincifying
Co Ni Mn Cu Zn Mg Na Ca Other
3.1 9.8 50.1 0.0015 0.005 13.7 66 0.6 ≦0.01
Dezincification slag ingredient %
Zn Mn Ni Cu Co
50.1 10.1 0.2 0.3 0.6
Solution after dezincifying liquid caustic soda maintains about the pH4.0 of solution, adds Sodium Fluoride according to calcium magnesium mol ratio 1:1.5, maintains temperature of reaction 85 DEG C, and stirring reaction filters for 2 hours, filtrate and filter residue composition as follows.
Liquid composition g/l after calcium-magnesium removing
Co Ni Mn Cu Zn Mg Na Ca Other
3.1 9.7 50.0 0.0015 0.005 0.003 85 0.002 ≦0.01
Filter residue analytical results %
Ca Mg Ni Mn Co Zn
7.2 35.1 0.01 0.3 0.01 0.01
Get P204 extraction agent (20%P204+80% sulfonated kerosene), use liquid caustic soda saponification, saponification degree 60%, 8 stage countercurrent extractions, 4 stage countercurrent washings, 8 stage countercurrent back extractions are simulated with separating funnel, charging pH4.0, wash the sulfuric acid of acid for 0.5mol/l, sour regurgitation is the sulfuric acid of 2mol/l, feed liquid: P204: wash acid: sour regurgitation=1:5:0.15:0.6(volume flow ratio), the strip liquor finally obtained and raffinate analytical results are as following table.
Strip liquor composition g/l
Co Ni Mn Cu Zn Mg Na Ca Other
5.3 16.5 79.5 0.0025 0.008 0.005 0.002 0.005 ≦0.002
Raffinate ingredient m g/l
Co Ni Mn Cu Zn
1.2 2.1 0.2 0.2 0.1
Filtrate after P204 enrichment is added sulfuric acid and maintain reaction about pH2.0, add manganese sulfide, temperature of reaction 50 DEG C according to zinc-copper mol ratio 1:5, react after 2 hours and filter, the filtrate obtained is as following table.
Ternary liquid g/l after the degree of depth dezincifies
Co Ni Mn Cu Zn Mg Na Ca Other
5.2 16.3 79.5 0.0012 0.003 0.005 0.002 0.005 ≦0.002
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (6)

1. a cobalt metallurgy of nickel waste water slag recycling processing method, is characterized in that: comprise following step:
1) reducing leaching
According to solid-to-liquid ratio 1:2-6 by waste water slag pulp, add the pH 1-2 that acid maintains reaction, add reductive agent according to cobalt manganese mol ratio 1:0.5-4 simultaneously, stirring reaction 1-3 hour at 50-70 DEG C, oxygenant is added according to iron mol ratio 1:0.1-0.6, add the pH3.5-5.5 of alkali regulator solution, stir after 1-4 hour and filter;
2) manganese powder displacement copper
Filtrate after removal of impurities is added acid for adjusting pH 1-3, adds manganese powder according to copper mol ratio 1:1.05-1.5, maintain temperature of reaction 40-80 DEG C, stirring reaction 1-3 hour;
3) manganese sulfide dezincifies
Filtrate after copper removal is added acid and maintain reaction pH 1-3, add manganese sulfide according to zinc mol ratio 1:1.1-1.5, temperature of reaction 40-80 DEG C, react after 1-3 hour and filter;
4) fluorochemical calcium-magnesium removing
Solution after dezincifying alkaline solution maintains the pH 3-6.5 of solution, adds fluorochemical, maintain filtration in temperature of reaction 50-90 DEG C, stirring reaction 1-3 hour according to calcium magnesium mol ratio 1:1.2-2.0;
5) P 20 4extracting and enriching
Get P 20 4extraction agent (10-30% P 20 4+ 70-90% sulfonated kerosene), use alkaline solution saponification, saponification degree 50-75%, with the extraction of separating funnel simulation 6-9 stage countercurrent, the washing of 4-6 stage countercurrent, the back extraction of 8-10 stage countercurrent, charging pH 3.5-5.5, washes the sulfuric acid of acid for 0.5mol/l, sour regurgitation is the sulfuric acid of 2mol/l, feed liquid: P 20 4: wash acid: sour regurgitation=1:4-8:0.1-0.3:0.4-0.8(volume flow ratio);
6) the manganese sulfide degree of depth dezincifies
Filtrate after P204 enrichment is added sulfuric acid and maintain reaction pH1-3, add manganese sulfide according to zinc-copper mol ratio 1:5, temperature of reaction 50 DEG C, react after 1-3 hour and filter.
2. a kind of cobalt metallurgy of nickel waste water slag recycling processing method according to claim 1, it is characterized in that: in described step 1, acid is at least one in sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid, reductive agent is at least one in sulfurous acid, sulphite, oxygenant is at least one in hydrogen peroxide, oxymuriate, oxygen, and alkali is at least one in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor.
3. a kind of cobalt metallurgy of nickel waste water slag recycling processing method according to claim 1, is characterized in that: in described step 2, acid is at least one in sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid.
4. a kind of cobalt metallurgy of nickel waste water slag recycling processing method according to claim 1, is characterized in that: in described step 3, acid is at least one in sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid.
5. a kind of cobalt metallurgy of nickel waste water slag recycling processing method according to claim 1, it is characterized in that: in described step 4, alkali is at least one in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor, fluorochemical is at least one in Potassium monofluoride, Sodium Fluoride, Neutral ammonium fluoride, hydrogen fluoride.
6. a kind of cobalt metallurgy of nickel waste water slag recycling processing method according to claim 1, is characterized in that: in described step 5, alkali is at least one in sodium hydroxide, potassium hydroxide, hydrated barta, ammoniacal liquor.
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CN105206889A (en) * 2015-07-29 2015-12-30 刘嘉因 Treatment method for waste LiMn1-x-yNixCoyO2 ternary battery cathode material
CN107058745A (en) * 2017-04-21 2017-08-18 青海快驴电动汽车科技有限公司 A kind of method that valuable metal is extracted in cobalt metallurgical waste
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CN107385217A (en) * 2017-08-02 2017-11-24 贵州轻工职业技术学院 The processing method of metal waste liquid and the method for reclaiming metal
CN108265178A (en) * 2018-03-08 2018-07-10 蒋央芳 A kind of processing method of cobalt metallurgy of nickel waste water slag
CN108977652A (en) * 2018-09-12 2018-12-11 郑忆依 A kind of resource utilization method of the waste water slag of cobalt metallurgy of nickel
CN109231181A (en) * 2018-11-26 2019-01-18 广东佳纳能源科技有限公司 Processing method, ternary precursor, battery-grade iron phosphate and the lithium ion battery of iron vitriol dreg of yellow sodium
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CN109250803A (en) * 2018-11-29 2019-01-22 黄河水利职业技术学院 A kind of electroplating waste processing equipment and processing method
CN109536732A (en) * 2018-12-13 2019-03-29 江西赣锋循环科技有限公司 A method of ternary precursor material is prepared using vulcanization copper ashes recycling
CN110512080A (en) * 2019-09-12 2019-11-29 金川集团股份有限公司 Valuable metal separation and recovery method in a kind of waste and old nickel cobalt manganese lithium ion battery
CN110629034A (en) * 2019-09-16 2019-12-31 厦门钨业股份有限公司 Method for recovering cobalt and nickel from tungsten waste recovery slag
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CN111455171A (en) * 2019-01-22 2020-07-28 深圳市金航深海矿产开发集团有限公司 Method for extracting valuable metals from seabed polymetallic nodules and co-producing lithium battery positive electrode material precursor and titanium-doped positive electrode material
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CN105206889A (en) * 2015-07-29 2015-12-30 刘嘉因 Treatment method for waste LiMn1-x-yNixCoyO2 ternary battery cathode material
WO2017162038A1 (en) * 2016-03-25 2017-09-28 邹传军 Method for removing calcium and magnesium ions from deep-processed plant product
CN107058745A (en) * 2017-04-21 2017-08-18 青海快驴电动汽车科技有限公司 A kind of method that valuable metal is extracted in cobalt metallurgical waste
CN107385217A (en) * 2017-08-02 2017-11-24 贵州轻工职业技术学院 The processing method of metal waste liquid and the method for reclaiming metal
CN108265178A (en) * 2018-03-08 2018-07-10 蒋央芳 A kind of processing method of cobalt metallurgy of nickel waste water slag
CN108977652B (en) * 2018-09-12 2019-11-22 郑忆依 A kind of resource utilization method of the waste water slag of cobalt metallurgy of nickel
CN108977652A (en) * 2018-09-12 2018-12-11 郑忆依 A kind of resource utilization method of the waste water slag of cobalt metallurgy of nickel
CN109231181A (en) * 2018-11-26 2019-01-18 广东佳纳能源科技有限公司 Processing method, ternary precursor, battery-grade iron phosphate and the lithium ion battery of iron vitriol dreg of yellow sodium
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CN111455171B (en) * 2019-01-22 2021-10-08 深圳市金航深海矿产开发集团有限公司 Method for extracting valuable metals from seabed polymetallic nodules and co-producing lithium battery positive electrode material precursor and titanium-doped positive electrode material
CN111455171A (en) * 2019-01-22 2020-07-28 深圳市金航深海矿产开发集团有限公司 Method for extracting valuable metals from seabed polymetallic nodules and co-producing lithium battery positive electrode material precursor and titanium-doped positive electrode material
CN110512080A (en) * 2019-09-12 2019-11-29 金川集团股份有限公司 Valuable metal separation and recovery method in a kind of waste and old nickel cobalt manganese lithium ion battery
CN110629034A (en) * 2019-09-16 2019-12-31 厦门钨业股份有限公司 Method for recovering cobalt and nickel from tungsten waste recovery slag
CN110669933A (en) * 2019-10-21 2020-01-10 金驰能源材料有限公司 Method for removing fluorine in nickel-cobalt-manganese solution
CN111471864A (en) * 2020-04-24 2020-07-31 广东邦普循环科技有限公司 Method for recovering copper, aluminum and iron from waste lithium ion battery leachate
CN111471864B (en) * 2020-04-24 2022-02-18 广东邦普循环科技有限公司 Method for recovering copper, aluminum and iron from waste lithium ion battery leachate
CN114182109A (en) * 2020-09-14 2022-03-15 北京博萃循环科技有限公司 Nickel-cobalt feed liquid extraction impurity removal process and device thereof
CN112499686A (en) * 2020-12-18 2021-03-16 杜长福 Method for preparing aluminum-doped battery-grade manganese oxyhydroxide by using waste manganese liquid
CN114487263A (en) * 2021-12-31 2022-05-13 宜宾光原锂电材料有限公司 Method for determining content of nickel, cobalt and manganese in nickel, cobalt and manganese-containing waste
CN114487263B (en) * 2021-12-31 2023-08-08 宜宾光原锂电材料有限公司 Method for measuring nickel cobalt manganese content in nickel cobalt manganese-containing waste

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